Sodium borohydride → HCID 15895427, Verbindung

HRID 1457225Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1457225
[CH3:1][C:2]1[C:3]([N:8]([CH2:31][O:32][CH2:33][CH2:34][O:35][CH3:36])[S:9]([C:12]2[C:13]([C:18]3[CH:23]=[CH:22][C:21]([C:24]4[O:25][CH:26]=[CH:27][N:28]=4)=[CH:20][C:19]=3[CH:29]=[O:30])=[CH:14][CH:15]=[CH:16][CH:17]=2)(=[O:11])=[O:10])=[N:4][O:5][C:6]=1[CH3:7].[BH4-].[Na+]>CO>[CH3:1][C:2]1[C:3]([N:8]([CH2:31][O:32][CH2:33][CH2:34][O:35][CH3:36])[S:9]([C:12]2[C:13]([C:18]3[CH:23]=[CH:22][C:21]([C:24]4[O:25][CH:26]=[CH:27][N:28]=4)=[CH:20][C:19]=3[CH2:29][OH:30])=[CH:14][CH:15]=[CH:16][CH:17]=2)(=[O:11])=[O:10])=[N:4][O:5][C:6]=1[CH3:7]

Komponenten

4

Edukt 2

HCID 4311764Sodium borohydrideHCID 15895425HCID 15895425, Verbindung

Produkt 1

HCID 15895427HCID 15895427, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of the title compound of step D (0.37 g, 0.76 mmol) in 10 mL of MeOH at room temperature, sodium borohydride (0.035 g, 0.93 mmol) was added and the mixture stirred for 2 hours. The clear solution was then concentrated to 5 mL and diluted with 100 mL of water and the aqueous solution was extracted with 3×100 mL of EtOAc. The combined organic extracts were then washed once with water and dried and evaporated to provide 0.3 g (95%) of the title compound of this step as a colorless gum.

Aufarbeitung

  1. concentrationThe clear solution was then concentrated to 5 mL
  2. additiondiluted with 100 mL of water
  3. extractionthe aqueous solution was extracted with 3×100 mL of EtOAc
  4. washThe combined organic extracts were then washed once with water
  5. customdried
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-8d738fd2fe4842f88e3d4d4239a4c7c2
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05846990

Notizen zur Reaktion

Wird geladen…